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 Troubleshooting 

Agilent Sample Introduction Pump System SIPS 10/20 User’s Guide 

73 

 

8.

 

Troubleshooting 

Two Pumps Not Connected 

74 

SIPS 10 

74 

SIPS 20 

74 

Pump Calibration Failed! Switch to Single  

Pump Operation 

74 

Dual Pump SIPS or Diluter Required to  

Prepare Standard Additions 

75 

Unable to Achieve Blank Reading 

75 

No Flame Detected – SIPS Operation Cannot Continue  76 
Dilution Factor > 50 

76 

Dilution factor > 200 

76 

LRR Calibration Failed – Default LRR Value Used 

77 

SIPS Offline or Pump Not Connected 

77 

The SIPS Doesn't Pump 

77 

The Absorption Signal Drifts Over Time 

78 

Poor Sensitivity 

78 

Poor Precision 

79 

There are Spikes in the Absorbance Signal 

79 

The Accuracy of the Result is Poor 

79

 

 

This chapter discusses the various SIPS related error messages, and 
offers solutions to problems you may encounter while using SIPS. If 
the suggestions provided do not resolve the problem, or if you 
encounter other problems with SIPS, contact your local Agilent office 
or field service engineer for assistance. 

 

 

Содержание SIPS 10

Страница 1: ...Agilent Sample Introduction Pump System SIPS 10 20 User s Guide...

Страница 2: ...e hardware and or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license Restricted Rights Legend If software is...

Страница 3: ...Hazard Warnings 10 Electrical Hazards 10 Moving Parts Hazard 11 Chemical Hazards 11 Other Precautions 11 Notes and Tips 11 Warning Symbols 12 Information Symbols 13 Color Coding 13 CE Compliance 13 El...

Страница 4: ...ump Unit and Electronic Control Module 28 Cabling 30 Connecting to the Agilent AA Computer 30 Connecting to the SIPS Unit 30 Installing the Pump Bands 32 Installing the Diluent Tubing 33 Connecting th...

Страница 5: ...a Single Standard 44 SIPS 10 44 SIPS 20 45 Automatic Calibration and Dilution of Overrange Samples 46 SIPS 10 46 SIPS 20 47 Autorun with QC Spikes SIPS 20 48 Online Addition of Chemical Modifier or In...

Страница 6: ...indow 64 Options Page 64 Analysis Window 64 Calibrate Pumps 64 Determine SIPS LRR 65 Flame Facilities Dialog 65 Load 65 Unload 65 Purge RH Pump 66 Purge LH Pump 66 Stop Pumps 66 Flame Optimization 66...

Страница 7: ...ble to Achieve Blank Reading 75 No Flame Detected SIPS Operation Cannot Continue 76 Dilution Factor 50 76 Dilution factor 200 76 LRR Calibration Failed Default LRR Value Used 77 SIPS Offline or Pump N...

Страница 8: ...Contents 8 Agilent Sample Introduction Pump System SIPS 10 20 User s Guide This page is intentionally left blank...

Страница 9: ...n of the Sample Introduction Pump System SIPS accessory involves the use of high voltage and moving parts Careless improper or unskilled use of this accessory can cause death or serious injury to pers...

Страница 10: ...ologies assumes no liability for the customer s failure to comply with these requirements Hazard Warnings In addition to the hazard warnings specified in your spectrometer operation manual specific ha...

Страница 11: ...governing the use handling and disposal of hazardous materials are strictly observed These safety practices should include wearing the appropriate safety clothing Always ensure that the sample introdu...

Страница 12: ...es a warning The meanings of the symbols that may appear alongside warnings in the documentation or on the instrument itself are as follows Corrosive liquid Electrical shock Fire hazard Hot surface Mo...

Страница 13: ...color coded to represent the status of the instrument or accessory A green light indicates the instrument is in normal standby condition A blue light indicates that operator intervention is required A...

Страница 14: ...Class A equipment is equipment suitable for use in all establishments other than domestic and those directly connected to a low voltage power supply network which supplies buildings used for domestic...

Страница 15: ...devices are also certified 5 Make sure that appropriate cables are used to connect the device to peripheral equipment 6 Consult your equipment dealer Agilent Technologies or an experienced technician...

Страница 16: ...Safety Practices and Hazards 16 Agilent Sample Introduction Pump System SIPS 10 20 User s Guide This page is intentionally left blank...

Страница 17: ...ions for the control module can be ignored It is still necessary to unpack and install the SIPS pump module The unique range of capabilities and applications provided by the SIPS includes Online 10 po...

Страница 18: ...tion of modifiers CAUTION The SIPS is not suitable for use with organic solvents because the tubing is not resistant to these solvents Figure 1 The SIPS 10 single pump unit The SIPS 10 uses a single p...

Страница 19: ...y regulated facilitating online standard additions calibration spiking of samples and addition of modifiers Samples can still be diluted online by reducing the sample pump speed relative to the speed...

Страница 20: ...aining the SIPS It is intended for use by laboratory personnel responsible for the day to day use of an Agilent AA instrument fitted with a SIPS unit The manual does not include instructions for setti...

Страница 21: ...llowing categories Installation category II Pollution degree 2 Equipment class I Condition Altitude Temp t C Humidity RH non condensing Non operating transport 0 2133 m 0 7000 ft 5 45 20 80 Operating...

Страница 22: ...0 Hz 1 Hz Consumption 70 W NOTE For safety reasons any other internal fuse or circuit breaker is not operator accessible and should be replaced only by an Agilent field service engineer External Conne...

Страница 23: ...14 2 in Unpacked pump module electronic control module2 275 285 215 mm 10 8 11 2 8 5 in 225 100 385 mm 8 9 4 15 2 in Performance Typical dilution error is 2 Guaranteed performance based on 3 3 second...

Страница 24: ...Specifications 24 Agilent Sample Introduction Pump System SIPS 10 20 User s Guide This page is intentionally left blank...

Страница 25: ...lizer 33 Installing the SIPS Pump Tubing 33 Extending the Pump Tubing 35 Calibrating the SIPS Pressure Arm Force 35 Conditioning the SIPS Pump Tubing 38 Fitting the Dust Cover 38 Connection to an Auto...

Страница 26: ...connect the pump unit to the electronic control module refer to Page 30 Install the pump bands refer to Page 32 Prepare rinse and diluent solutions of 0 01 Triton X 100 refer to Page 39 Install the SI...

Страница 27: ...of proper electrical grounding can create a fire or shock hazard that can cause death serious injury or serious damage to equipment Do not connect the SIPS to the mains power until you have checked t...

Страница 28: ...e cap out carefully the fuse should be held in the fuseholder in the fuse cap 4 Check that the fuse is the correct type and is not damaged If necessary replace the fuse in the holder 5 Place the fuse...

Страница 29: ...an Agilent 280FS AA or 140 240 AA3 the electronic module is built into the instrument If so you will not need to follow the steps for installing this module To attach the electronic control module to...

Страница 30: ...te port is clearly labeled and the other end to the port on the back of the computer For Agilent 50 55 AA instruments which do not require a computer plug the IEEE 488 cable into the IEEE port on the...

Страница 31: ...routed around the bottom edge of the instrument or underneath it CAUTION The SIPS is not suitable for use with organic solvents because the tubing is not resistant to these solvents NOTE If you are u...

Страница 32: ...n the left side of the T piece as shown in Figure 4 Figure 4 Installing the pump band and tubing on the SIPS 10 20 NOTE If you are installing pump bands on a SIPS 10 there is only one roller The follo...

Страница 33: ...ure head The use of any other diluent vessel may introduce dilution errors Connecting the SIPS to the Nebulizer Use a 15 mm piece of silicone tubing 1 mm ID as supplied with the SIPS to connect the up...

Страница 34: ...range tab to hold the tubing in position 6 Fit the tube around the left side of the roller drum positioning it between the presser arm and the pump band 7 Hook the tube into the rear slot in the press...

Страница 35: ...lled or after the SIPS has been repaired by an Agilent field service engineer This procedure may be completed by the service engineer at the time of installation NOTE This must be carried out using a...

Страница 36: ...only one SIPS Arm Force field 6 Click Load Arm to start the SIPS operating Observe if the de ionized water in the inlet line starts to pulse or flow up the line If the liquid in the tube is not moving...

Страница 37: ...water Place the outlet tube of the capillary in an empty beaker 4 Light the flame 5 Access the Service diagnostic page 54 by holding the Alt key down while you type 54 on the numeric keypad This page...

Страница 38: ...to 15 minutes and press OK Pump this solution until the time has lapsed 3 Replace the detergent solution with de ionized water and pump for an additional 30 minutes This will complete the conditioning...

Страница 39: ...s pass into the flame Replacing the Pump Tubing When you need to replace the pump tubing you should follow these additional maintenance procedures and operational 1 Release the plastic pump band s fro...

Страница 40: ...ing an alcohol moistened cloth wipe the pump rollers Ensure they all free of corrosion and dirt and rotate freely 8 Clean the nebulizer and Pt Ir capillary using the standard procedure shown in the Sp...

Страница 41: ...s chapter assumes you have correctly set up your spectrometer and optimized the system for flame operation The examples in this chapter are for the PC based SpectrAA system refer to the online Help fo...

Страница 42: ...ure that the bulk standard has been accurately prepared This will determine the accuracy of your calibration and your sample results Make the calibration cover an extended Absorbance range approaching...

Страница 43: ...ner to warm up and stabilize Nebulizer Setup For correct operation of the SIPS it is essential that the nebulizer uptake rate is correctly adjusted The following procedure must be performed each time...

Страница 44: ...f the nebulizer blocks replace the diluent in the Mariotte vessel because blocking causes the flow of sample to be reversed towards the Mariotte vessel leading to contamination of the diluent and inco...

Страница 45: ...ges as required and click OK 7 Switch to the Analysis window 8 Ensure the diluent tubing is connected to the Mariotte vessel then select Calibration from the Instrument menu Select the method you want...

Страница 46: ...s window select the required Smart rinse on overrange error action and the required Flush time for the Smart rinse This is the error action that is executed if any contamination is detected after an o...

Страница 47: ...SIPS 20 To perform overrange dilution using SIPS 20 1 Develop or modify a method as described for SIPS 10 with the following exception on the SIPS page select Bulk Standard in the Right Pump group 2...

Страница 48: ...IPS pumps forward at full speed for a short period then reduces the pump speed to automatically dilute the sample If any contamination is remaining after 30 s an error message appears and the SIPS Pur...

Страница 49: ...Smart rinse on overrange error action and the required Flush time for the Smart rinse 7 Click OK and switch to the Analysis window 8 Ensure the diluent tubing is connected to the Mariotte vessel and...

Страница 50: ...er Uptake Rate and the modifier Pump speed in the Right Pump group according to the amount of modifier or Internal standard you wish to add to your samples NOTE To prevent the contamination of the dil...

Страница 51: ...prompted The second pump automatically adds the modifier to the sample on line in the quantity specified in the method NOTE The speed of the modifier pump will remain constant throughout the analysis...

Страница 52: ...se only one pump of the SIPS 20 unit 1 Develop or modify a method according to the instructions for the SIPS 10 see the Automatic Calibration from a Single Standard section on Pages 44 45 of this manu...

Страница 53: ...ndard Additions as the calibration mode 4 On the SIPS page a Select Bulk Standard from the Right Pump group If you will be running a very long autorun with many samples it may be necessary to periodic...

Страница 54: ...it in the first sample and press Read The top addition standard will be checked first to see if it is within the linear reading range at maximum pump speed If the absorbance of the highest addition s...

Страница 55: ...ion 5 On the Standards page enter the concentrations of the pre mixed standards in the table as per non SIPS operation NOTE The Bulk standard concentration and the Standard count is disabled since the...

Страница 56: ...Read This will check the top standard addition to see if it is within the linear reading range at maximum pump speed 12 At the next prompt place the pump tubing inlet in the reagent blank and press R...

Страница 57: ...w 64 Options Page 64 Analysis Window 64 Calibrate Pumps 64 Determine SIPS LRR 65 Flame Facilities Dialog 65 Load 65 Unload 65 Purge RH Pump 66 Purge LH Pump 66 Stop Pumps 66 Flame Optimization 66 Star...

Страница 58: ...tic online overrange sample dilution Measurement Page Two values are relevant to SIPS operation on the Measurement page in the Method window Read Delay This field defines the time required to pump sol...

Страница 59: ...utton if you have a SIPS 10 unit or are not going to use the second pump of a SIPS 20 unit Bulk Standard Select this radio button if you want to use the second pump on the SIPS 20 to perform all calib...

Страница 60: ...eed of the second pump relative to the first pump on the SIPS 20 unit Refer to the previous section Modifier for details NOTE The actual pump speed is dynamic and will change depending upon the value...

Страница 61: ...elevant method in the autorun and the value in the Linear reading range field is used You can either accept the default LRR value or enter your own Calibration Mode Autoset Standard Concentrations In...

Страница 62: ...odically recalibrate the pumps during a long autorun to correct for any possible drift which may have occurred particularly if there is any significant difference in the ages of the sample pump tubing...

Страница 63: ...Default is off the Concentration column in the Standards table will be unavailable The SIPS will calculate the concentration of the standards from the Bulk standard concentration and the Standard coun...

Страница 64: ...lank reading appears and the error action selected in this list is executed Analysis Window The following SIPS functions are available in the Analysis window Calibrate Pumps Selecting Calibrate pumps...

Страница 65: ...e methods This will only be available for those methods where SIPS is selected AND the calibration mode selected is standard additions Flame Facilities Dialog Selecting Flame Facilities from the Analy...

Страница 66: ...Purge LH Pump Pressing this button runs the pump for the rinse time specified in the method to flush out standard or modifier from the tubing of the left pump This button is enabled for a SIPS 20 uni...

Страница 67: ...d surfaces The acid residue may also be activated by moisture on the hands of the next person to touch that surface For details of fuse replacement refer to Page 27 Daily If a new pump tube has been f...

Страница 68: ...d there are no leaks If necessary cut the ends of the tubing by a small amount to improve the connection When the tubing becomes too short replace the tubing Inspect the pump tubing before each run If...

Страница 69: ...min Adjust the nebulizer to increase the uptake rate e g adjust the capillary so that it is closer to the high vac position Alternatively and if it is not possible to increase the nebulizer uptake ra...

Страница 70: ...o longer acceptable in terms of accuracy and precision this is an indication that the pump bands should be replaced Once replaced repeat the measurement If this still has not restored the accuracy pre...

Страница 71: ...ventilation slots on the rear of the instrument Check that the connecting cable from the power module to the SIPS pump module is secured If not disconnect and refit When complete switch the power bac...

Страница 72: ...Maintenance 72 Agilent Sample Introduction Pump System SIPS 10 20 User s Guide This page is intentionally left blank...

Страница 73: ...factor 200 76 LRR Calibration Failed Default LRR Value Used 77 SIPS Offline or Pump Not Connected 77 The SIPS Doesn t Pump 77 The Absorption Signal Drifts Over Time 78 Poor Sensitivity 78 Poor Precisi...

Страница 74: ...cond pump is correct on the SIPS page Pump Calibration Failed Switch to Single Pump Operation The error message Pump Calibration failed Switch to single pump operation appears during an autorun The SI...

Страница 75: ...ding The error message Unable to achieve blank reading appears during an autorun This error message will appear if the final absorbance reading during a Smart Rinse fails to fall below the user define...

Страница 76: ...encounter this message if you attempt to start SIPS without the flame on or if the flame goes out while SIPS is pumping This is to prevent the contamination of the diluent which occurs if SIPS is all...

Страница 77: ...hod but do not have a SIPS unit installed correctly Ensure all cabling to the SIPS is connected properly Turn the SIPS off and on again to reset communications The SIPS Doesn t Pump Ensure that the fl...

Страница 78: ...inse make up and diluent solutions at a concentration of 0 01 If using a SIPS 20 select periodic pump recalibration particularly if running many samples Check the nebulizer or capillary for blockage b...

Страница 79: ...d completely over the barb The Accuracy of the Result is Poor Ensure that you are using the pump tubes supplied and recommended by Agilent you are using one of the Agilent supplied Marriotte vessels t...

Страница 80: ...gnal Check the nebulizer or capillary for blockage by disconnecting the capillary from the T piece to see if any signal is obtained when SIPS is bypassed Rectify if required Check the uptake rate of t...

Страница 81: ......

Страница 82: ...ribes the following Safety Practices and Hazards Introduction Specifications Installation Operation Command Reference Maintenance Troubleshooting Agilent Technologies 1999 2000 2010 2012 2016 2017 07...

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